KING KHALID UNIVERSITY

COLLEGE OF PHARMACY

DEPARTMENT OF PHARMACOLOGY

COURSE SCHEDULE

MALE SECTION

ANALYTICAL CHEMISTRY - II (PCH 320)

FOR

PHARMACEUTICAL SCIENCES / CLINICAL PHARMACY

BY

Dr. SYED TASQEERUDDIN

Academic Session 1437-38 H

1st Semester

(Semester No 371)

September 2016 - January 2017

COURSE SPECIFICATION

Course title PHARMACEUTICAL ANALYTICAL

CHEMISTRY-II

Course code PCH-320

Credit hours 3+1 credit units (60 hrs)

3 Theory and 1 Practical per week

Program(s) in which the course is

offered

BACHELOR OF PHARMACEUTICAL

SCIENCES / CLINICAL PHARMACY

Name of faculty member responsible for

the course

Dr. Syed Tasqeeruddin

Assistant Professor

Room No: 164/4/C

Department of Pharmaceutical chemistry

College of Pharmacy-King Khalid

University, ABHA.

Office: 024177982

hsyed@kku.edu.sa

Mobile No:0596051708

Lecture Timings Theory Wednesday: 09:00 – 10:00 AM Room No: C/34/4

Thursday: 09:00 –10:00 AM Room No: C/34/4

Lecture Timings Practical Sunday: 01:00– 03:00PM,

Tuesday: 02.00– 04:00PM,

Level/year at which this course is offered 5th Level / 3rd Year

Pre-requisites for this course (if any) PCH-219

Co-requisites for this course (if any) Not Applicable

Location if not on main campus

Total number of teaching weeks 15 Weeks

Total number of lectures Theory 45 Hours

Total number of Practical Hours 60 Hours

Course Description:

The course presents the basis and applications of instrumental analytical techniques:

UV-visible spectrophotometry, Fluorometry, FTIR, Atomic Absorption

Spectrophotometry, Flame Photometry, ICP-AES and Mass Spectrometry, Voltammetry,

Potentiometry, Ponductometry, Separation techniques, Chromatography (Liquid

chromatography - TLC - High-performance liquid chromatography (HPLC) – Gas

chromatography), Electrophoresis.

THE MAIN LEARNING OUTCOMES FOR STUDENTS ENROLLED IN THE COURSE

TEXT BOOK FOR REFERENCE

1. Providing the students with knowledge of various modern methods of

instrumental techniques in order to prepare them for industrial or academic

careers. The course stresses quantitative and qualitative analysis using modern

instrumental analytical techniques. These techniques are applied for analysis of

organic, inorganic compounds and pharmaceutical compounds.

2. The instrumental methods include optical, electrometric and chromatographic

methods of analysis.

1. Principles of Instrumental Analysis, Fifth Edition, Douglas A. Skoog, F. James

Holler, Timothy A. Nieman, Harcourt Brace College Publishers, 1998.

2. Analytical Chemistry for Technicians, Third Edition, John Kenkel, CRC Press,

LLC, 2003.

SCHEDULE OF ASSESSMENT TASKS

EXAMINATION PROTOCOL:

QUIZ EXAM

It will consist 10 multiple choice questions for 05 marks

Topics for Quiz Exam

Quiz examination will take place in 4th teaching week; Date will be announced

through Black Board as per the agreement with group leader.

MID-TERM EXAM

24 MCQs = 01 x 24 = 24 Marks

3 Short Answers out of 5 = 02 x 03 = 06 Marks

Total = 30 Marks

Quiz exam 05 Marks

Mid Term Theory Exam 30 Marks

E- Assignments 05 Marks

Mid Term practical Exam 10 Marks

Final practical Exam 10 Marks

Final Exam 40 Marks

Total 100 Marks

1. General introduction to the Instrumental methods of analysis and their importance in

pharmaceutical studies. Introduction to Spectrophotometric Analysis – Regions of

Electromagnetic spectrum – Interaction of light with matter, Basic components of

spectrophotometers – Absorption of radiation by molecules - Concept of quantization of energy

2. UV/Visible Absorption Spectra of compounds - Transmittance and Absorbance - Beer’s law -

Deviations from Beer's Law, Types of electronic transition - Chromophoric Groups – Factors

affecting absorption spectra - Selection of the suitable Wavelength for Spectrophotometric

analysis.

Topics for Mid-term exam

FOR MID TERM EXAMINATION, DATE, TIME AND PLACE OF EXAMINATION

WILL BE INFORMED BY ACADEMIC OFFICE.

Assignments through E-Learning Activity:

It will be given individually to the students from the topics of the course to do some

online activities in the black board. It will carry 05 marks.

END SEMSTER EXAM

Final exam will consist of 80 multiple choice questions for 40 marks.

The mcqs will be from the topics covered from 6th teaching week onwards.

DURATION OF EXAMINATION IS 2 HOURS

FOR END SEMESTER EXAMINATION, DATE, TIME AND PLACE OF

EXAMINATION WILL BE INFORMED BY ACADEMIC OFFICE

MIDTERM EXAMINATION SYLLABUS INCLUDES TOPICS COVERED IN ANY

FIVE WEEKS OF THE TEACHING SCHEDULE

TEACHING SCHEDULE FOR PHARMACEUTICAL ANALYTICAL

CHEMISTRY - II – PCH – 320 – THEORY

Teaching

Week NO

Course content Date / Day Name of the Faculty

1 1. Optical Spectrometry-I

UV/Visible Spectrophotometry - Fundamentals of

Spectrophotometry - Properties of Light (Wavelength

Frequency, velocity of Light, Energy of radiations)

Regions of the electromagnetic spectrum –Absorption

of Light - Molecular processes (Rotation – Vibration –

Electronic transitions)

21-09-2016 /

WEDNESDAY

Dr. SYED

TASQEERUDDIN

Basic Components of Spectrophotometrs (Light Source

–Monochromator (Prism and diffraction grating) -

Sample Holder – Detector (Photomultiplier Tube and

Photodiode Array detector))

Types of Spectrophotometers: Single-Beam

Spectrophotometer and Double-Beam

Spectrophotometer - advantages of double-beam

spectropotometer over single beam instrument.

22-09-2016

THURSDAY

Dr.SYED

TASQEERUDDIN

2 2. Fourier Transform Infrared (FTIR) Spectroscopy

IR Spectroscopy (dispersive type) – The IR regions of

electromagnetic spectrum (Near, Mid and Far-IR) -

Wavenumber and Wavelength - Infrared Dispersive

Spectrometers - IR spectrum and interpretation.

What information can FT-IR provide – Why Fourier

transform infrared spectroscopy is preferred over

dispersive or filter methods of infrared spectral

analysis? – What is FT-IR?

28-9-2016

WEDNESDAY

Dr. SYED

TASQEERUDDIN

Instrumentation of FTIR (The Source - The

beamsplitter – The Interferometer - The Sample holder

- The Detector - The Computer) - FTIR Spectra - FTIR

Applications (Materials Evaluation - Verification

Analysis - Quality Control Screening - Basic and

29-9-2016

THURSDAY

Dr. SYED

TASQEERUDDIN

Applied Research

3 3. Optical Spectrometry-II

Transmittance and absorbance – Beer - Lambert’s law

Molar absorptivity - Quantitative spectrophotometric

analysis (calibration curve method - Analysis of

Binary Mixture) When Beer’s Law Fails (non-

obedience of Beer’s Law) : Fundamental cause of

deviation – Chemical deviation – Instrumental

Deviation

5-10-2016/

WEDNESDAY

Dr. SYED

TASQEERUDDIN

What Happens When a Molecule Absorbs Light? -

Chromophore Groups - Electronic transitions.

Optimum Conditions for Spectrophotometric

Measurements - Sample Conditions (Solvent Effect -

Cut-off of Solvents - Concentration and Pathlength) -

Instrumental Parameters (Slitwidth - Scanning Speed -

Stray light)

6-10-2016/

THURSDAY

Dr. SYED

TASQEERUDDIN

4 Chemical Derivatisation (Reasons of applying

Chemical derivatisation - Some Common Methods of

Chemical treatments and Derivatisation (Metal-Ligand

Complexation - Diazotisation and coupling of primary

aromatic amines - Condensation Reactions - Reduction

of tetrazolium salts - The acid-dye method))

Spectrophotometric Applications for pharmaceutical

Analysis (UV/Visible spectra – Determination of pKa

values – Determination of solubility and partition

coefficients of drugs – Release of drug from

formulation)

12-10-2016 /

WEDNESDAY

Dr. SYED

TASQEERUDDIN

4. Molecular Emission Spectroscopy

Molecular Fluorescence and Phosphorescence Spectra

- Energy level diagram for a molecule showing

pathways for deactivation of an excited state -

Radiationless Deactivation (Vibrational relaxation (vr)

- internal conversion (ic) - External conversion -

Intersystem crossing (isc))

13-10-2016

THURSDAY

Dr. SYED

TASQEERUDDIN

5 Relaxation with Emission of photons (Fluorescence -

Phosphorescence) -Quantum yield, f - Instrumental

components of Spectrofluorimeter (The basic design of

spectrofluorimeter and the most significant differences

between spectrofluorimeter and spectrophotometer)

19-10-2016/

WEDNESDAY

Dr. SYED

TASQEERUDDIN

Relation between Absorption and Emission Spectra -

Quantitative relation between the intensity of

fluorescence & concentration - Fluorescence Intensity

and quantitative applications - Factors Affecting

fluorescence intensity (Dissolved Oxygen – pH -

Temperature - Viscosity of solvent - Quenchers )

20-10-2016

THURSDAY

Dr. SYED

TASQEERUDDIN

6 Fluorescence and Structure (Aromaticity – Conjugation

Degree of rings condensation - Effect of Structural

Rigidity - Effect of Substitution on fluorescence)–

Fluorimetric applications involving non- fluorescent

analytes - Advantages of Molecular photoluminescence

over absorption spectrophtometr.

26-10-2016/

WEDNESDAY

Dr. SYED

TASQEERUDDIN

5. Electroanalytical Techniques

1. Potentiometry (Nernst equation - Reference

Electrode (Calomel Electrodes - Silver/Silver Chloride

Electrodes - Indicator Electrodes)

Ion Selective Electrodes - Membrane Electrodes and

membrane potentials - The glass membrane electrode -

Mechanism of action and selectivity to H+ in glass

membrane.

27-10-2016/

THURSDAY

Dr. SYED

TASQEERUDDIN

7 Crystalline Solid-State Ion-Selective Electrodes: Ag+

ion selective electrode, Fluoride ion-selective

Electrode; Liquid-membrane Ion-Selective Electrodes,

Ca2+

-selective electrode, Potentiometric Biosensors -

Urea electrode. Analytical Applications of Ion-

Selective Electrodes, Quantitative Analysis Using

External Standards, Measurement of pH, Clinical

2-11-2016/

WEDNESDAY

Dr. SYED

TASQEERUDDIN

Applications Environmental Applications –

Potentiometric Titration

6. Atomic absorption spectroscopy (AAS)

Atomization processes - absorption of radiation by

these free atoms - Flame atomization and Flame

Processes - Absorption spectra. Basic Components of

Atomic Absorption Spectrometer

Source of radiation (Hollow Cathode Lamp) –

Sputtering process and emitting spectral lines specific

for analyte being measured.

3-11-2016 /

THURSDAY

Dr. SYED

TASQEERUDDIN

8 Atomization Unites (Flame Atomization Unit (Premix

Burner) - Electrotherma Atomization (Graphite

Furnace) - Cold Vapour Technique - Hydride

Generation Technique). Quantitative Applications

(Calibration Curve) – Interferences (Chemical –

Physical and Spectral interferences) – Methods of

minimizing or eliminating interferences (matrix

matching - Standard Addition Method - Chemical

treatment)

9-11-2016/

WEDNESDAY

Dr. SYED

TASQEERUDDIN

7.Voltammetry

Fundamental studies involving the use of voltammetry

– Polarography (The Polarographic Cell -

Polarographic Measurements - limiting diffusion

current Id - half wave potential (E½) – Voltammogram.

Reduction and Oxidation (Redox) Processes - Ilkovic

equation- Advantagesand disadvantages of DME as a

working electrode

10-11-2016 /

THURSDAY

Dr. SYED

TASQEERUDDIN

9 Stripping Voltammetry (Anodic stripping voltammetry

- Cathodic stripping voltammetry - Adsorptive

stripping voltammetry). Cyclic Voltammetry (The

controlling potential- excitation signal - The cyclic

voltammogram- Reduction peak- Oxidation peak -

peak current – peak separation)

16-11-2016 /

WEDNESDAY

Dr. SYED

TASQEERUDDIN

8. Atomic Emission Spectrometry

(Excitation and Emission spectra - Flame Photometry –

Instrumentation and Applications

17-11-2016 /

THURSDAY

Dr. SYED

TASQEERUDDIN

10 Inductively Coupled Plasma Atomic Emission

Spectrometry (ICP-AES) - ICP Torch - Temperature of

the ICP - ICP-AES Instrumentation - Sample

Introduction and nebulization - Sequential and

simultaneous determinations.

Pharmaceutical Application of Atomic Spectrometry

23-11-2016 /

WEDNESDAY

Dr. SYED

TASQEERUDDIN

9.MassSpectrometry

What is Mass Spectrometry? - m/z ratio – Use of Mass

Spectrometry (Atomic Mass Spectrometry - Molecular

Mass Spectrometry - Principle components of mass

spectrometer and basic steps)

24-11-2016 /

THURSDAY

Dr. HISSANA

ATHER

11 Sample introduction systems (Direct Vapor Inlet -

Direct Insertion Probe (DIP - Gas Chromatography

inlet system - Liquid Chromatography inlet system)-

Ion sources (Electron source (EI) - Chemical Ionization

(CI) - Atmospheric Pressure Ionization (API) and

Electrospray Ionization - Matrix Assisted Laser

Desorption/Ionization (MALDI)- Fast Atom

Bombardment (FAB)

30-11-2016 /

WEDNESDAY

Dr. SYED

TASQEERUDDIN

a) Mass Analyzers (Quadrupole - Magnetic Sector-

Time-of-Flight Mass Analyzer)

b) Detectors (photographic plates - photomultiplier

tube) Vacuum systems d) Data System

1-12-2016/

THURSDAY

Dr. SYED

TASQEERUDDIN

12 Interpretation of mass spectra. 7-12-2016 /

WEDNESDAY

Dr. SYED

TASQEERUDDIN

10. Chromatography

Phases of Chromatography (the mobile phase - the

stationary phase) - Tswett’s Experiment -

8-12-2016/

THURSDAY

Dr. SYED

TASQEERUDDIN

chromatogram Classification of chromatographic

methods. Types of stationary phases in column

chromatography (adsorption, partition, ion exchange, and

size exclusion) - The retention time, tR.

13 Liquid Chromatography - Planer Chromatography -

Paper chromatography and (Ascending Paper

Chromatography - Descending Paper Chromatography

- Two-dimensional Paper Chromatography - Retention

Factor, Rf - Interpreting the data - Thin Layer

Chromatography

14-12-2016/

WEDNESDAY

Dr. SYED

TASQEERUDDIN

Instrumental Chromatography - high-performance

liquid chromatography - The basic components of

HPLC system (Solvent reservoirs - high-pressure pump

- Injection device - Guard column - The analytical

column - The detector - Data system) - Mobile Phase in

HPLC - Isocratic Elution - Gradient elution - Sample

Injection. Types of HPLC Columns - Normal Phase

Columns (NP HPLC) - mobile phases for NP HPLC -

Stationary phase for NP HPLC - Bonded stationary

phases – Applications of NP HPLC.

Reverse Phase Columns (RP HPLC) - Mobile phases

for RP HPLC - Stationary Phases in RP-HPLC - –

Applications of RP HPLC.

15-12-2016/

THURSDAY

Dr. SYED

TASQEERUDDIN

14 Gas Chromatography (carrier gas - Gas

Chromatography System - vapor pressure and sequence

of separation in GC - Gas Chromatography Columns -

Types of GC columns (Packed column, and Open-

tubular capillary column - Open-tubular capillary

column - The Nature of the Stationary Phase in GC.

Gas Chromatography Detectors (Thermal Conductivity

Detector - Flame Ionization Detector - Electron

Capture Detector - Mass Spectromety and Infrared

Detectors - GC application in drug analysis. Gas

21-12-2016/

WEDNESDAY

Dr. SYED

TASQEERUDDIN

Chromatography Detectors (Thermal Conductivity

Detector - Flame Ionization Detector - Electron

Capture Detector - Mass Spectromety and Infrared

Detectors - GC application in drug analysis.

Chiral Chromatography (Types of Chiral Stationary

Phases - formation of transient diastereomeric and

separation strategy)

22-12-2016

THURSDAY

Dr. SYED

TASQEERUDDIN

15 REVISION 28-12—2016

WEDNESDAY

Dr. SYED

TASQEERUDDIN

REVISION 29-12-2016

THURSDAY

Dr. SYED

TASQEERUDDIN

TEACHING SCHEDULE FOR PHARMACEUTICAL ANALYTICAL

CHEMISTRY – II – PCH – 320 – PRACTICAL

Group A, Monday, 08.00–10.00 AM; Lab No C/2/20

Week Date Topic

Faculty Name

1 25-09-2016 Construction of absorption spectrum

curve of chemical compound.

Dr. SYED

TASQEERUDDIN

2 2-10-2016 Spectrophotometric determination of Mn

in KMnO4 solution

‘’

3 9-10-2016 Quantitative Analysis of Aspirin Tablets

by Ultraviolet Absorption

Spectrophotometry

‘’

4 16-10-2016 The Spectrophotometric Determination

of Iron in Natural Water

“

5 23-10-2016 Two component analysis ( Colorimetric

analysis of Co2+ & Ni2+ mixture)

“

6 30-10-2016 Fluoro metric determination of Quinine

“

7 6-11-2016 Revision “

8

13-11-2016

Practical Examination – I “

9 20-11-2016 Potentiometric titration of HCl against

NaOH

“

10 27-11-2016 Conductometric titration of HCl against

NaOH

“

11 4-12-2016 Thin-layer chromatographic separation of

amino acids.

“

12 11-12-2016 Demonstration on HPLC and GC instruments “

13 18-12-2016 “

14 25-12-2016 Revision “

15 1-01-2017 Practical Examination – II “

TEACHING SCHEDULE FOR PHARMACEUTICAL ANALYTICAL

CHEMISTRY – II – PCH – 320 – PRACTICAL

Group B, Wednesday, 08.00–10.00 AM; Lab No C/2/20

Week Date Topic

Faculty Name

1 27-09-2016 Construction of absorption spectrum

curve of chemical compound.

Dr. SYED

TASQEERUDDIN

&

Dr. Vel

2 4-10-2016 Spectrophotometric determination of Mn

in KMnO4 solution

“

3 11-10-2016 Quantitative Analysis of Aspirin Tablets

by Ultraviolet Absorption

Spectrophotometry

“

4 18-10-2016 The Spectrophotometric Determination of

Iron in Natural Water

“

5 25-10-2016 Two component analysis ( Colorimetric

analysis of Co2+ & Ni2+ mixture)

“

6 1-11-2016 Fluoro metric determination of Quinine

“

7 8-11-2016 Revision

“

8 22-11-2016 Practical Examination – I

“

9 29-11-2016 Potentiometric titration of HCl against NaOH

“

10 6-12-2016 Conductometric titration of HCl against

NaOH

“

11 13-12-2016 Thin-layer chromatographic separation of

amino acids.

“

12 20-12-2016 Demonstration on HPLC and GC instruments

“

13 27-12-2016

“

14 3-1-2016 Practical Examination – II “